AVS2011 Session HI+AS+BI+NS-WeM: Nano- and Bio- Imaging with Helium Ion Microscopy

Wednesday, November 2, 2011 8:40 AM in 106

Wednesday Morning

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8:40 AM HI+AS+BI+NS-WeM-3 Helium Ion Microscopy Techniques for Imaging and Characterization of nano-Device Materials and Structures
Shinichi Ogawa, Tomohiko Iijima (National Institute of Advanced Industrial Science and Technology (AIST), Japan)

This paper presents several imaging modes for nano-devices fabrication that may make HIM a tool of particular value to soft materials such as low-k dielectrics (low-k) with less transformation and more materials contrast which reflects damaged areas, and copper interconnect buried in dielectrics, and shows luminescence induced by the focused helium ion beam using the HIM for the first time.

Imaging of -100 nm pitch patterned low-k is important for LSI Cu/low-k interconnect processes, while SEM imaging results in changes to the low-k line edge roughness and shape by damage during an electron beam irradiation. The HIM could provide low-k dielectric secondary electron (SE) image with nm order resolution, deeper focus depth, less transformation because of three order magnitude lower thermal energy transfer into a unit volume of the low-k than the SEM under an appropriate operation condition1).

During the imaging, even at very low helium ion current, surfaces of samples were atomically etched off, as in a graphene patterning, and then blistering or physical etch occurred with the increase of the helium ion current. This makes the interpretation of the HIM SE imaging difficult but helpful. Damaged areas at side walls of the low-k regions in a 140 nm pitch interconnect were successfully seen with a different contrast from non-damaged low-k regions at an “optimized” helium ion beam condition2), which was similar to a TEM/Valence EELS result. On the other hand, using the SEM, the damaged areas contrast in the low-k regions could not been imaged.

A new imaging mode, through the inter-level dielectric, of the underlying copper, was explored. Cu interconnect was seen through a 130 nm thick low-k dielectrics. The incident helium ions might generate secondary electrons(SEs) at the buried Cu surface and the SEs of 1-2 eV energy passed through the dielectric of a few eV band gap without any energy transfer, and then the image was obtained. Helium ion channeling at the Cu surface area varied the secondary electron quantity, and it might generate a crystal orientation contrast of the buried Cu metal.

Luminescence induced by the focused helium ion beam was studied using the HIM2). Helium ion beam of a few pA current was irradiated to a SiO2 film, and peaks in a spectrum were observed at around 281, 447, and 672 nm; these positions were different from those by a conventional SEM cathode luminescence. The further study will be presented.

L.Stern, W.Thompson and J.Nottte of Carl Zeiss are acknowledged for their discussions in the Cu / low-k works.

1) S. Ogawa, et al, Jpn. J. Appl. Phys., 49 (2010) 04DB12, 2) S. Ogawa, et al, Proc. of 2011 IEEE IITC (2011)

9:20 AM HI+AS+BI+NS-WeM-5 He Ions Image the Au (111) Herringbone Reconstruction
Vasilisa Veligura, Gregor Hlawacek, Raoul van Gastel, Harold Zandvliet, Bene Poelsema (MESA+ Institute for Nanotechnology, University of Twente, Enschede, The Netherlands)
The herringbone reconstruction of the Au(111) surface was directly visualized using an Ultra High Vacuum Helium Ion Microscope. Ion channeling phenomena arise from the different atomic ordering in the outermost layer of the crystal. First, we investigated the channeling contrast from the bulk Au fcc structure by imaging polycrystalline Au on glass films. The contrast that was observed as a function of crystal orientation was found to conform to what is calculated from a simple hard sphere model. Consequently, the herringbone reconstruction was investigated. It is a periodic zigzag structure of the three different types of crystal stacking (fcc, hcp and bridge sites connecting these regions) and, ideally, has a period of 6.3 nm. The different stacking of the atoms that constitute the surface reconstruction leads to lateral variations of the secondary electron yield that can be resolved in HIM imagery. The existence of the herringbone reconstruction on the sample was independently confirmed through STM measurements and the quantitative details from both techniques are similar, but seem to be affected by the differences in vacuum conditions. An influence of both the ion beam and vacuum environment on the visibility of the herringbone reconstruction is observed in our UHV-HIM system.
9:40 AM HI+AS+BI+NS-WeM-6 Imaging of Graphenoid Nanomembranes with Helium-Ion Microscopy
André Beyer, Andrey Turchanin, Armin Gölzhäuser (University of Bielefeld, Germany)

Helium-ion microscopy is known for its high surface sensitivity. Here we present a study about imaging extremely thin nano-scale objects: graphenoid nanomembranes which consist exclusively of atoms near the surface. Such freestanding nanomembranes with a thickness of 1 nm are made from self-assembled monolayers (SAMs) by cross-linking and subsequent transfer to transmission electron microscopy (TEM) grids or other suitable substrates. We show that these nanomembranes exhibit a substantially higher contrast in helium-ion microscopes as compared to electron microscopes.

Cross-linking of SAMs is performed by large area exposures with electrons or photons which yield extended nanomembranes. On the other hand, patterned exposures allow the fabrication of nanosieves, i.e. perforated nanomembranes. Advantages in imaging such patterned cross-linked SAMs as well as freestanding nanosieves with the helium-ion microscope will be discussed.
10:00 AM BREAK - Complimentary Coffee in Exhibit Hall
10:40 AM HI+AS+BI+NS-WeM-9 Nanofabrication and Biological Imaging with the Helium Ion Microscope
Daniel Pickard (National University of Singapore)

The Helium Ion Microscope (HIM) is a new imaging technology based on a high brightness and stable Gas Field Ion Source (GFIS). The GFIS employed exhibits a low energy spread (<1 eV), small virtual source size (< 0.3 nm) and a high brightness > 4 x 109 A/cm2.sr [1]. This, in conjunction with the shallow escape depth (<1 nm) of the secondary electrons generated by the incident 30 keV helium ions, contribute to the HIM’s primary advantage in the imaging of solid samples: its high spatial resolution (0.25 nm) [2]. We have applied this novel technology across a broad spectrum of multidisciplinary applications (from basic materials science and semiconductor applications to the biological sciences) to assess its utility and possible advantages over alternative techniques.

One area where our investigations have gained significant traction is in the imaging of biological specimens. The utility of this instrument in addressing topics of the biological sciences is due in part to the HIM’s high spatial resolution. However, in the context of biological specimens, it is the ability to image non-conductive samples without the application of a metal (or other conductive) overcoat and without the need of a background gas (both of which degrade resolution and surface details), which has proven to be a distinguishing attribute. This opens up a whole new range of biological problems that can be solved rapidly and with less risk of artifacts.

An equally compelling application is in the field of nano-structuring. The focused helium ions have the ability to directly modify the sample surface under a high ion flux (via surface sputtering). This enables the direct patterning of structures and promises great utility in the fabrication of sub-10 nm devices. It also provides a mechanism for high resolution patterning on nonconventional substrates (such as suspended graphene membranes), where resist-based lithographic techniques are not feasible. Our experiences in sub-10 nm pattern transfer for both graphene and plasmonics applications will be presented.

1. B. Ward, J. Notte, and N. Economou, J. Vac. Sci. Technol. B, Vol. 24, No. 6, Nov/Dec 2006

2. Application Note, Carl Zeiss SMT, “Ultra-High Resolution Imaging in ORION®PLUS”, PI No. 0220-2008-ENG, Nov. 21, 2008

11:20 AM HI+AS+BI+NS-WeM-11 Imaging and Characterizing Cellular Interaction of Nanoparticles using Helium Ion Microscopy
Bruce Arey, Vaithiyalingam Shutthanandan, Yumie Xie, Ana Tolic, Galya Orr (Pacific Northwest National Laboratory)
The helium ion mircroscope (HeIM) probes light elements (e.g. C, N, O, P) with high contrast due to the large variation in secondary electron yield, which minimizes the necessity of specimen staining. A defining characteristic of HIM is its remarkable capability to neutralize charge by the implementation of an electron flood gun, which eliminates the need for coating non-conductive specimens for imaging at high resolution. In addition, the small convergence angle in HeIM offers a large depth of field (~5x FE-SEM), enabling tall structures to be viewed in focus within a single image. Taking advantage of these capabilities, we investigate the interactions of engineered nanoparticles (NPs) at the surface of alveolar type II epithelial cells grown in culture. The increasing use of nanomaterials in a wide range of commercial applications has the potential to increase human exposure to these materials, but the impact of such exposure on human health is still unclear. One of the main routs of exposure is the respiratory tract, where alveolar epithelial cells present a vulnerable target. Since the cellular interactions of NPs govern the cellular response and ultimately determine the impact on human health, our studies will help delineating relationships between particle properties and cellular interactions and response to better evaluate NP toxicity or biocompatibility.

The Rutherford backscattered ion (RBI) is a helium ions imaging mode, which backscatters helium ions from every element except hydrogen, with a backscatter yield that depends on the atomic number of the target. Energy-sensitive backscatter analysis is being developed, which when combined with RBI image information, support elemental identification at helium ion submicron resolution. This capability will enable distinguishing NPs from cell surface structures with nanometer resolution.

11:40 AM HI+AS+BI+NS-WeM-12 Application of Helium Ion Microscope on Semiconductor Surface Imaging and Metrology
Hongxuan Guo (National Institute for Materials Science, Japan); Hiroshi Itoh (National Institute of Advanced Industrial Science and Technology (AIST), Japan); Keiko Onishi, Tamaki Iwasaki, Daisuke Fujita (National Institute for Materials Science, Japan)

Scanning electron microscope (SEM) has been used in the semiconductor surface imaging and metrology for more than 50 years. Now, a new tool, Helium ion microscope (HeIM), is developed and applied to this work. SEM and HeIM are the same in some fundamental characteristics. But, the latter has advantages in smaller probe size, higher resolution, and greater depth of field. These abilities enhance the performance of the HeIM in the semiconductor surface imaging and metrology, such as imaging of low–k materials [1] and measurement of critical dimension of the semiconductor devices [2].

A standard sample for scanning probe microscope tip characterization [3, 4] was measured by using HeIM and atomic force microscope (AFM) as shown in Fig. 1 and Fig. 2. Line profile of the HeIM image in Fig. 1 shows high accuracy in edge definition of the sample. The contrast of the image is related to morphology and materials of the sample [5], the probe size of the Helium ion beam, direction of the sample and beam, charge distribution, and so on. All the aspects will be analyzed in our presentation. The AFM image of the sample shown in Fig. 2 is a dilation of the real surface topography of the sample due to the finite-size AFM tip [6]. With an erosion algorithm, the surface of the sample was reconstructed to be compared with HeIM measurement.

[1] S. Ogawa, W. Thompson, L. Stern, L. Scipioni, J. Notte, L. Farkas , and L. Barriss, Jpn. J. Appl. Phys., 49, 04DB12(2010)

[2] M. T Postek , A. Vladar , C. Archie and B. Ming, Meas. Sci. Technol., 22, 024004 (2011)

[3] H. Itoh, C. Wang, H. Takagi, Proc. of SPIE, 7971, 79711A-1, (2011).

[4] H. Takenaka, M. Hatayama, H. Ito, T. Ohchi, A. Takano, S. Kurosawa, H. Itoh, and S. Ichimura, Journal of Surface Analysis, 17, 264, (2011).

[5] Y. Sakai, T. Yamada, T. Suzuki, T. Sato, H. Itoh, and T. Ichinokawa, Appl. Phys. Lett., 73, 611 (1998)

[6] M. Xu, D. Fujita, and K. Onishi, Rev. Sci. Instrum., 80, 043703 (2009)

Time Period WeM Sessions | Abstract Timeline | Topic HI Sessions | Time Periods | Topics | AVS2011 Schedule